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Ethanolamine → HCID 86737404、化合物

HRID 355014
ノート
印刷プレビュー

反応式

HRID 355014 の反応式
[C:1]12[C:14](=[O:15])[O:13][C:11](=O)[C:2]=1[CH2:3][CH2:4][C:5]1[C:10]2=[CH:9][CH:8]=[CH:7][CH:6]=1.[CH2:16]([CH2:18][NH2:19])[OH:17]>C(O)(=O)C>[OH:17][CH2:16][CH2:18][N:19]1[C:11](=[O:13])[C:2]2[CH2:3][CH2:4][C:5]3[C:10]([C:1]=2[C:14]1=[O:15])=[CH:9][CH:8]=[CH:7][CH:6]=3
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 700EthanolamineHCID 1422143,4-Dihydro-1,2-naphthalenedicarboxylic anhydride

生成物 1

HCID 86737404HCID 86737404、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 70 g (0.35 mol) of 3,4-dihydronaphthalene-1,2-dicarboxylic acid anhydride [prepared according to Org. Syntheses, Col., Vol. 2, 194 (1943)] and 23.5 g (0.385 mol) of ethanolamine in 1.7 liters of glacial acetic acid is kept under reflux for 24 hours. The glacial acetic acid is then removed by distillation, the residue is dissolved in 2 liters of absolute ethanol, 50 g of an ion exchanger ("Dowex 50 W" from Fluka AG) are added and the suspension is kept under reflux for 24 hours. The ion exchanger is then filtered off, the ethanol is distilled off and the residue is recrystallised from diethyl ether/ethanol. This yields 61.8 g (73% of theory) of N-(2'-hydroxyethyl)-3,4-dihydronaphthalene-1,2-dicarboximide; melting point 120.5°-121° C.

後処理

  1. temperatureunder reflux for 24 hours
  2. customThe glacial acetic acid is then removed by distillation
  3. dissolutionthe residue is dissolved in 2 liters of absolute ethanol
  4. addition50 g of an ion exchanger ("Dowex 50 W" from Fluka AG) are added
  5. temperatureunder reflux for 24 hours
  6. filtrationThe ion exchanger is then filtered off
  7. distillationthe ethanol is distilled off
  8. customthe residue is recrystallised from diethyl ether/ethanol

出典と根拠

ORDレコード
ord-b067f255d8aa443abf7b912c560a7d69
出典データセット
uspto-grants-1983_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04377669

反応ノート

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